Dissolve 50.00 g (0.36 mol) of 2,4- dimethylbenzenethiol (5) in 300 mL of DMF, add 30.44 g () of potassium hydroxide and stir at room temperature.
0.5425mol) of potassium hydroxide, stir at room temperature, add a total of 56.99 g (0.3617 mol) of o-chloronitrobenzene (6) in 3 batches, and react at 50 .
The reaction was carried out at 50 for 5 h. The reaction was monitored by thin-layer chromatography (TLC), and the unfolding reagent was [ ethyl acetate: petroleum ether (AR bp: 60 ~90 )=1:5] .
The reaction was monitored by TLC. After the reaction was completed and cooled to room temperature, 900 mL of distilled water was added with thorough stirring, a large amount of solid was precipitated, and the filter cake was filtered and recrystallized with ethanol to obtain 89.10 g of compound 4. Yield 95%, mp: 98.0%.
95%, mp: 98 ~100 , MS: C 14 H 13 NO 2 S [M+Na] + 282.0563 .
